StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Methanol → 1-Butyl-3-methoxypyridine-2-thione

HRID 416562
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 416562
[CH2:1]([N:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][CH3:12])[C:6]1=O)[CH2:2][CH2:3][CH3:4].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1.CO>C1(C)C=CC=CC=1>[CH2:1]([N:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][CH3:12])[C:6]1=[S:23])[CH2:2][CH2:3][CH3:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 887MethanolHCID 87949Lawesson's reagentHCID 105593101-Butyl-3-methoxy-2-pyridone

Produkt 1

HCID 222665361-Butyl-3-methoxypyridine-2-thioneAusbeute 80,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a solution of 1-butyl-3-methoxy-2-pyridone (2-034-02) (6.4 g) in toluene (150 mL) was added Lawesson's reagent (16.8 g), and the reaction mixture was heated under reflux. After the reaction mixture was stirred for 3 h, to the reaction mixture was added methanol (100 mL), and the reaction mixture was stirred for 30 min. After the solvent was evaporated under reduced pressure, to the reaction mixture were added water and ethyl acetate, and the organic layer was separated. The aqueous layer was extracted three times with ethyl acetate, and the combined organic layers were washed with water and brine, dried over anhydrous magnesium sulfate, and evaporated under reduced pressure. The crude product was purified by silica gel column chromatography to give 1-butyl-3-methoxypyridine-2-thione (2-034-03) (5.6 g, 80%) as an oil.

Aufarbeitung

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux
  3. stirringthe reaction mixture was stirred for 30 min
  4. customAfter the solvent was evaporated under reduced pressure, to the reaction mixture
  5. additionwere added water and ethyl acetate
  6. customthe organic layer was separated
  7. extractionThe aqueous layer was extracted three times with ethyl acetate
  8. washthe combined organic layers were washed with water and brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customevaporated under reduced pressure
  11. customThe crude product was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-89abf018af6c48b0aa09f424b1bf3a1e
Quelldatensatz
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08088924B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion